LU82072A1 - GRANULATION PROCESS FOR TRANS-D1-1-HYDROXY-3- (1 ', 1'-DIMETHYLHEPTYL) -6,6-DIMETHYL-6A, 7,8,9,10,10A-HEXAHYDROBENZO (B, D) PYRAN -9-ONE (NABILONE) - Google Patents

GRANULATION PROCESS FOR TRANS-D1-1-HYDROXY-3- (1 ', 1'-DIMETHYLHEPTYL) -6,6-DIMETHYL-6A, 7,8,9,10,10A-HEXAHYDROBENZO (B, D) PYRAN -9-ONE (NABILONE) Download PDF

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Publication number
LU82072A1
LU82072A1 LU82072A LU82072A LU82072A1 LU 82072 A1 LU82072 A1 LU 82072A1 LU 82072 A LU82072 A LU 82072A LU 82072 A LU82072 A LU 82072A LU 82072 A1 LU82072 A1 LU 82072A1
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LU
Luxembourg
Prior art keywords
nabilone
ethanol
trans
hydroxy
dimethyl
Prior art date
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LU82072A
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French (fr)
Inventor
J Conine
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Lilly Co Eli
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Application filed by Lilly Co Eli filed Critical Lilly Co Eli
Publication of LU82072A1 publication Critical patent/LU82072A1/en

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/33Heterocyclic compounds
    • A61K31/335Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
    • A61K31/35Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/141Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/146Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic macromolecular compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/08Drugs for disorders of the alimentary tract or the digestive system for nausea, cinetosis or vertigo; Antiemetics

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  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Public Health (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Veterinary Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Organic Chemistry (AREA)
  • Otolaryngology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • General Chemical & Material Sciences (AREA)
  • Hospice & Palliative Care (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Pyrane Compounds (AREA)

Description

_ --Ï »_ --Ï "

La nabilone [trans-dl-l-hydroxy-3-(1',1’-diméthyl-heptyl)-6,6-diméthyl-6a,7,8,9,10,10a-hexahydrobenzo[b,d[pyran- 9-one] fait partie d'un groupe d'intermédiaires utiles =· préparés par Farenholtz, et al·, J. Am. Chem. Soc., 88, 2079 5 (1966) , 8_9, 5934 (1967) pour la préparation du Δ^-THC (tetra- • hydrocannibinol) et de ses homologues alkylés comportant des groupements alkyle de 1 à 10 atomes de carbone sur le carbone 9 C-3. (Δ -THC est le trans-dl-l-hydroxy-3-n-pentyl-6,6,9-trimëthyl-6a,7,8,10a-têtrahydrobenzo[b,d]pyrrane). Dans les 10 brevets des E.U.A. N° 3.928.598, 3.953.603, 3.946.673 et * 3.998.188, Archer indique que la nabilone, en plus d'être un "intermédiaire utile", a une activité comme médicament antidépresseur, anti-anxiété, analgésique et/ou sédatif, et Archer et Lemberger ont en outre étendu ces actions utiles à 15 celle d'anti-émétique et à l'action pour le traitement des glaucomes, voir les brevets des E.U.A. N° 4.087.545 et 4.087.547. La nabilone n'est pas bien absorbée par l'intestin pendant l'administration orale. Thakker et al., J. Pharm. Pharroac., 29, 783 (1977) décrivent certaines compositions 20 utiles de la nabilone, comprenant une dispersion dans la polyvinylpyrrolidinone. Thakker et al. mélangent la nabilone avec la PVP dans un rapport de 1:2-20 dans un solvant comme l'éthanol puis chassent le solvant par évaporation sous vide. Le produit ainsi obtenu est un solide vitreux qui doit 25 d'abord être brisé puis réduit en une poudre fine pour le disperser uniformément dans d'autres excipients pharmaceutiques avant son introduction dans des capsules de gélatine s'emboîtant.Nabilone [trans-dl-1-hydroxy-3- (1 ', 1'-dimethyl-heptyl) -6,6-dimethyl-6a, 7,8,9,10,10a-hexahydrobenzo [b, d [pyran - 9-one] is part of a group of useful intermediaries = · prepared by Farenholtz, et al ·, J. Am. Chem. Soc., 88, 2079 5 (1966), 8_9, 5934 (1967) for the preparation of Δ ^ -THC (tetra- • hydrocannibinol) and its alkylated counterparts having alkyl groups of 1 to 10 carbon atoms on the carbon 9 C-3. (Δ -THC is trans-dl-1-hydroxy-3-n-pentyl-6,6,9-trimethyl-6a, 7,8,10a-tetrahydrobenzo [b, d] pyrran). In the 10 U.S. patents N ° 3.928.598, 3.953.603, 3.946.673 and * 3.998.188, Archer indicates that nabilone, in addition to being a "useful intermediary", has an activity like antidepressant drug, anti-anxiety, analgesic and / or sedative, and Archer and Lemberger have further extended these useful actions to that of antiemetic and to the action for the treatment of glaucoma, see US Patents N ° 4.087.545 and 4.087.547. Nabilone is not well absorbed from the intestine during oral administration. Thakker et al., J. Pharm. Pharroac., 29, 783 (1977) describe certain useful compositions of nabilone, comprising a dispersion in polyvinylpyrrolidinone. Thakker et al. mix the nabilone with the PVP in a ratio of 1: 2-20 in a solvent such as ethanol and then remove the solvent by evaporation under vacuum. The product thus obtained is a glassy solid which must first be broken up and then reduced to a fine powder in order to disperse it uniformly in other pharmaceutical excipients before its introduction into interlocking gelatin capsules.

Cette invention est un procédé permettant de 30 fournir une composition de granulation pour la nabilone qui évite les défauts et les difficultés de la dispersion solide * susmentionnée de Thakker et al.This invention is a method of providing a granulation composition for nabilone which avoids the defects and difficulties of the aforementioned solid dispersion * of Thakker et al.

En particulier, l'invention fournit une solution de nabilone et de polyvinylpyrrolidone dans l'éthanol, en tant 35 que solution de granulation. Cette solution est ensuite utilisée pour granuler des excipients et supports pharmaceutiques comme l'amidon, le lactose, la cellulose, etc. Après séchage et broyage, le matériau granulé en poudre i 2 peut être mélange avec d'autres matériaux pour préparer une composition que l'on peut introduire dans des capsules de gélatine s'emboîtant comme prévu. En d'autres termes, la dispersion nabilone-PVP de Thakker et al est formée in situ * 5 comme composant de granulation pour des excipients qui sont insolubles dans l'éthanol. Le rapport de la nabilone à la PVP, * dans la nouvelle composition de granulation comme dans les dispersions de Thakker et al, est de une partie de nabilone pour deux à vingt parties de PVP.In particular, the invention provides a solution of nabilone and polyvinylpyrrolidone in ethanol, as a granulation solution. This solution is then used to granulate excipients and pharmaceutical carriers such as starch, lactose, cellulose, etc. After drying and grinding, the granulated powder material i 2 can be mixed with other materials to prepare a composition which can be introduced into gelatin capsules which fit together as intended. In other words, the nabilone-PVP dispersion of Thakker et al is formed in situ * 5 as a granulation component for excipients which are insoluble in ethanol. The ratio of nabilone to PVP, * in the new granulation composition as in the dispersions of Thakker et al, is one part of nabilone for two to twenty parts of PVP.

10 Un produit de granulation ainsi préparé a une excellente stabilité en ce qui concerne la nabilone, et les * données de dissolution montrent que la granulation est équivalente à la dispersion de Thakker et al préparée sous forme d'un verre dans 1'évaporateur rotatif puis pulvérisée.A granulation product thus prepared has excellent stability with respect to nabilone, and the dissolution data show that the granulation is equivalent to the dispersion of Thakker et al prepared as a glass in the rotary evaporator and then sprayed.

15 On a montré chez les chiens une disponibilité biologique équivalente pour la composition granulée de cette invention par rapport à la dispersion de Thakker et al.Equivalent biological availability for the granulated composition of this invention has been shown in dogs compared to the dispersion of Thakker et al.

D'autres dispersions de nabilone préparées par Thakker et al, comprenant une dans le polyéthylèneglycol, 2 0 peuvent être préparées de même in situ sur l'exc.'. ient particulier en utilisant le nouveau procédé tel que décrit pour la dispersion de nabilone et de PVP ci-dessus : solution dans l'éthanol puis granulation d'un excipient insoluble dans 1'éthanol.Other dispersions of nabilone prepared by Thakker et al, including one in polyethylene glycol, can also be prepared in situ on exc. '. ient particular using the new process as described for the dispersion of nabilone and PVP above: solution in ethanol then granulation of an excipient insoluble in ethanol.

* 25 Cette invention est en outre illustrée par l'exemple spécifique suivant.* 25 This invention is further illustrated by the following specific example.

EXEMPLE 1EXAMPLE 1

On dissout cinq grammes de nabilone dans 125 ml d’éthanol anhydre et on y dissout 45 g de polyvinylpyrrolidone 30 (PVP). On ajoute la solution visqueuse résultante à 450 g de poudre fluide d'amidon dans un malaxeur Hobart. On utilise une petite quantité d'éthanol anhydre supplémentaire pour " introduire par rinçage le reste de la solution nabilone- PVP dans le malaxeur. Après un malaxage soigneux, on tamise 35 à l'état humide le produit granulé sur un tamis d’une ouverture de maille de 4,76 mm (on peut également utiliser un tamis d'une ouverture de maille de 3,36 mm).Le produit granulé tamisé est séché à l'air puis broyé jusqu'à la h r , 3 granulométrie désirée dans un broyeur à boulets.Five grams of nabilone are dissolved in 125 ml of anhydrous ethanol and 45 g of polyvinylpyrrolidone 30 (PVP) are dissolved therein. The resulting viscous solution is added to 450 g of fluid starch powder in a Hobart mixer. A small amount of additional anhydrous ethanol is used to "rinse" the remainder of the nabilone-PVP solution into the kneader. After careful kneading, the granulated product is sieved wet through an open sieve of 4.76 mm mesh (a sieve with a 3.36 mm mesh opening can also be used). The sieved granulated product is air dried and then ground to the hr, 3 desired particle size in a ball mill.

Une granulation nabilone-PVP-amidon ainsi préparée peut être ensuite mélangée a d'autres excipients pour obtenir un mélange final ayant la concentration désirée en nabilone * 5 en vue de son introduction dans des capsules de gélatine s'emboîtant vides.A nabilone-PVP-starch granulation thus prepared can then be mixed with other excipients to obtain a final mixture having the desired concentration of nabilone * 5 with a view to its introduction into empty interlocking gelatin capsules.

‘ On peut utiliser d'autres excipients insolubles dans l'éthanol, comme le lactose, le mannitol et le dextrose, à la place de l'amidon fluide pour préparer le produit granulé 10 précédent.‘Other excipients insoluble in ethanol, such as lactose, mannitol and dextrose, can be used in place of the fluid starch to prepare the preceding granulated product.

♦ ♦ 1 «♦ ♦ 1 "

Claims (2)

1. Procédé de préparation de la nabilone en vue de son administration par voie orale à des mammifères, caractérisé en ce qu'on dissout la nabilone et de la polyvinylpyrrolidone ·1 5 ou du polyéthylèneglycol dans de l'éthanol anhydre et on utilise la solution visqueuse ainsi formée pour granuler un ’ excipient insoluble dans l'éthanol et acceptable sur le plan pharmaceutique, par mélange soigneux de la solution avec l'excipient puis séchage du produit granulé ainsi formé.1. Process for the preparation of nabilone for oral administration to mammals, characterized in that the nabilone and polyvinylpyrrolidone · 1 5 or polyethylene glycol are dissolved in anhydrous ethanol and the solution is used viscous thus formed to granulate an excipient insoluble in ethanol and acceptable from a pharmaceutical point of view, by careful mixing of the solution with the excipient then drying of the granulated product thus formed. 2. Procédé selon la revendication 1, caractérisé en ce qu'on dissout de la polyvinylpyrrolidone et de la " nabilone dans l'éthanol pour former la solution de granulation. 2 4 22. Method according to claim 1, characterized in that polyvinylpyrrolidone and "nabilone are dissolved in ethanol to form the granulation solution. 2 4 2
LU82072A 1979-03-09 1980-01-10 GRANULATION PROCESS FOR TRANS-D1-1-HYDROXY-3- (1 ', 1'-DIMETHYLHEPTYL) -6,6-DIMETHYL-6A, 7,8,9,10,10A-HEXAHYDROBENZO (B, D) PYRAN -9-ONE (NABILONE) LU82072A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US1981079 1979-03-09
US06/019,810 US4195078A (en) 1979-03-09 1979-03-09 Nabilone granulation

Publications (1)

Publication Number Publication Date
LU82072A1 true LU82072A1 (en) 1980-04-23

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LU82072A LU82072A1 (en) 1979-03-09 1980-01-10 GRANULATION PROCESS FOR TRANS-D1-1-HYDROXY-3- (1 ', 1'-DIMETHYLHEPTYL) -6,6-DIMETHYL-6A, 7,8,9,10,10A-HEXAHYDROBENZO (B, D) PYRAN -9-ONE (NABILONE)

Country Status (16)

Country Link
US (1) US4195078A (en)
EP (1) EP0015635A1 (en)
JP (1) JPS55133309A (en)
AU (1) AU531805B2 (en)
BE (1) BE881049A (en)
CA (1) CA1124178A (en)
CH (1) CH643840A5 (en)
DK (1) DK8080A (en)
FR (1) FR2450606A1 (en)
GB (1) GB2045080B (en)
IE (1) IE49243B1 (en)
IL (1) IL59098A (en)
IT (1) IT1193886B (en)
LU (1) LU82072A1 (en)
NZ (1) NZ192557A (en)
ZA (1) ZA80104B (en)

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JPS59155309A (en) * 1983-02-22 1984-09-04 Teijin Ltd Active type vitamin d3 composition and its preparation
NZ211545A (en) * 1984-04-11 1987-09-30 Ici Australia Ltd Composition having particulate trace element suspended in matrix of solid polyethylene glycol
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CA2845443A1 (en) * 2014-03-04 2015-09-04 Pharmascience Inc. Orally disintegrating tablet of nabilone and method of manufacturing

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GB2045080A (en) 1980-10-29
BE881049A (en) 1980-07-09
CH643840A5 (en) 1984-06-29
ZA80104B (en) 1981-08-26
JPH0142923B2 (en) 1989-09-18
AU5455480A (en) 1980-09-11
AU531805B2 (en) 1983-09-08
IT1193886B (en) 1988-08-31
IT8019114A0 (en) 1980-01-09
DK8080A (en) 1980-09-10
FR2450606B1 (en) 1983-04-15
EP0015635A1 (en) 1980-09-17
IL59098A0 (en) 1980-05-30
GB2045080B (en) 1983-05-25
IE49243B1 (en) 1985-09-04
JPS55133309A (en) 1980-10-17
IE800042L (en) 1980-09-09
IL59098A (en) 1983-09-30
FR2450606A1 (en) 1980-10-03
NZ192557A (en) 1981-05-01
CA1124178A (en) 1982-05-25
US4195078A (en) 1980-03-25

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